US6530684B1 - Preparation of liquid dispersions - Google Patents
Preparation of liquid dispersions Download PDFInfo
- Publication number
- US6530684B1 US6530684B1 US09/455,135 US45513599A US6530684B1 US 6530684 B1 US6530684 B1 US 6530684B1 US 45513599 A US45513599 A US 45513599A US 6530684 B1 US6530684 B1 US 6530684B1
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- nozzle
- bore
- inlet
- nozzles
- turbulence chamber
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
- A61K9/1075—Microemulsions or submicron emulsions; Preconcentrates or solids thereof; Micelles, e.g. made of phospholipids or block copolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
- B01F25/421—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions by moving the components in a convoluted or labyrinthine path
- B01F25/422—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions by moving the components in a convoluted or labyrinthine path between stacked plates, e.g. grooved or perforated plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
- B01F25/452—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces
- B01F25/4521—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces the components being pressed through orifices in elements, e.g. flat plates or cylinders, which obstruct the whole diameter of the tube
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/06—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by singly-bound oxygen atoms
- C07C403/08—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by singly-bound oxygen atoms by hydroxy groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2215/00—Auxiliary or complementary information in relation with mixing
- B01F2215/04—Technical information in relation with mixing
- B01F2215/0413—Numerical information
- B01F2215/0418—Geometrical information
- B01F2215/0431—Numerical size values, e.g. diameter of a hole or conduit, area, volume, length, width, or ratios thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2215/00—Auxiliary or complementary information in relation with mixing
- B01F2215/04—Technical information in relation with mixing
- B01F2215/0413—Numerical information
- B01F2215/0436—Operational information
- B01F2215/0468—Numerical pressure values
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2215/00—Auxiliary or complementary information in relation with mixing
- B01F2215/04—Technical information in relation with mixing
- B01F2215/0413—Numerical information
- B01F2215/0436—Operational information
- B01F2215/0472—Numerical temperature values
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Definitions
- the present invention provides a process for mixing or dispersing liquids.
- a process for the production of a finely divided liquid dispersion is provided, as well as mixing devices for carrying out the process.
- European Patent Publication EP 0776 997 A1 describes a method for the production of a finely divided dispersion of solids in which a pre-dispersion is pumped through one or more slotted nozzles.
- the particle size of the dispersed phase lies in the region of 0.01 ⁇ m to 20 ⁇ m.
- the diameter of the nozzle bore is 0.05 mm to 1 mm.
- the ratio of bore length to bore diameter is 1:1 to 1:10.
- a preferred combination includes a device which has two nozzle bodies with the nozzles lying opposite their outlet. Also described are devices in which the crude dispersion or pre-dispersion is pumped through two or more nozzles having an equal or decreasing bore diameter.
- the slotted nozzle suitably consists of a ceramic material, for example, zirconium oxide, or a metal coated with ceramic.
- One embodiment of the invention is a process for mixing or dispersing liquids that includes introducing liquids to be mixed or dispersed into a mixing device having a cylindrical support.
- the cylindrical support includes an inlet nozzle having a bore which is in fluid communication through a turbulence chamber with a bore of an outlet nozzle, wherein the bores of the nozzles are axially spaced apart relative to one another.
- the liquids then enter the turbulence chamber through the bore of the inlet nozzle where the liquids are subjected to turbulence, i.e., are mixed or dispersed.
- the mixed or dispersed product is thereafter recovered from the outlet nozzle.
- FIG. 1 Another embodiment of the present invention is a mixing device having a cylindrical support.
- the cylindrical support includes an inlet nozzle having a bore which is in fluid communication through a turbulence chamber with a bore of an outlet nozzle, wherein the bores of the nozzles are axially spaced apart relative to one another.
- Another embodiment of the invention is a scale up arrangement wherein a plurality of nozzles are disposed within the cylindrical support.
- a further embodiment of the invention is a scale up arrangement that includes a first support disk, a turbulence chamber, and a second support disk, which are positioned in sequence in a conduit.
- the first support disk consists of a plurality of inlet nozzles having a bore diameter of about 0.05 mm to about 1 mm.
- the second support disk contains a plurality of outlet nozzles having a bore diameter of about 0.05 mm to about 1 mm.
- the bores of the inlet nozzles are in fluid communication with the bores of the outlet nozzles through the turbulence chamber and the bores of the inlet nozzles and outlet nozzles are axially spaced apart relative to one another.
- FIG. 1 shows a flow diagram for carrying out the process in accordance with the invention.
- FIG. 2 shows a cross section through a mixing device in accordance with the invention having an inlet nozzle and an outlet nozzle.
- FIG. 3 shows a perspective view of the mixing device in accordance with the invention.
- FIGS. 4 ( a-c ) shows a scale up arrangement.
- FIG. 5 shows another a scale up arrangement.
- the present invention solves the problem of the previously described devices by pumping the liquids to be mixed or to be dispersed at temperatures of about 20° C. to about 250° C., preferably of about 20° C. to about 200° C., and pressures of about 50 bar to about 2500 bar, preferably of about 100 bar to about 800 bar, through a mixing device which consists of one or more inlet nozzles, one or more turbulence chambers and one or more outlet nozzles, with the inlet nozzle(s), turbulence chamber(s) and outlet nozzle(s) being pressed in sequence in a cylindrical support.
- the bores of the inlet nozzles are in fluid communication with the bores of the outlet nozzles through the turbulence chamber and the bores of the inlet and outlet nozzles are axially spaced apart relative to one another.
- the process of the invention is especially suitable for the production of finely divided dispersions having average particle sizes of about 10 nm to about 1000 nm, preferably of about 50 nm to about 400 nm.
- a pre-emulsion is pumped through the aforementioned mixing device (dispersing unit).
- the pre-emulsion is at temperatures of about 20° C. to about 250° C., preferably of about 20° C. to about 200° C., and pressures of about 50 bar to about 2500 bar, preferably of about 100 bar to about 800 bar.
- the residence time of the liquids to be mixed or to be dispersed in the mixing device is about 10 ⁇ 6 sec to about 10 ⁇ 1 sec.
- pre-emulsion denotes one of the following systems:
- lipophilic active substance includes vitamins A, D, E and K, carotenoids, and food additives, such as PUFAs (polyunsaturated fatty acids) and tocotrienols.
- the liquid to be dispersed is preferably stirred into an aqueous emulsifier solution, optionally while warming.
- the processes for the production of finely divided liquid dispersions set forth herein relate not only to processes used in the food manufacturing field in which food emulsifiers are used, but also in general industrial dispersion processes in which corresponding industrial emulsifiers are used. Processes which are used in the food manufacturing field are preferred.
- suitable emulsifiers/stabilizers for dispersions which may be added to foods include, for example, ascorbyl palmitate, lecithins, polysorbates, sugar esters, fatty acid esters, citric acid esters, sorbitol stearates; as well as colloids, for example gelatines and fish gelatines; carbohydrates, for example starches and starch derivatives such as dextrin, pectin or gum arabic; milk proteins and plant proteins. Mixtures of the aforementioned substances can also be used. Ascorbyl palmitate, fish gelatines or starch derivatives are preferred, with ascorbyl palmitate being especially preferred.
- Suitable industrial emulsifiers are, for example, lauryl ethylene oxide (LEO)-9 and (LEO)-10.
- the process in accordance with the invention is especially suitable for the production of liquid dispersions from oils, such as, for example, corn oil, palm oil, sunflower oil, and the like.
- oils such as, for example, corn oil, palm oil, sunflower oil, and the like.
- the present process may also be used to produce liquid dispersions from lipophilic active substances, such as, for example, from vitamin A, D, E, and K, from carotenoids or from food additives such as PUFAs and tocotrienols.
- suitable carotenoids include, for example, beta-carotene, beta-apo-4′-carotenal, beta-apo-8′-carotenal, beta-apo-12′-carotenal, beta-apo-8′-carotenoic acid, astaxanthin, canthaxanthin, zeaxanthin, cryptoxanthin, citranaxanthin, lutein, lycopene, torularodin aldehyde, torularodin ethyl ester, neurosporaxanthin ethyl ester, zetacarotene, dehydroplectania-xanthin and the like.
- the aforementioned lipophilic active substances may be used directly insofar as they are oily substances.
- Solid active substances for example carotenoids, may also be used in dissolved form in oil or in water-immiscible solvents.
- Suitable water-immiscible solvents that may be used in the present invention include halogenated aliphatic hydrocarbons, such as for example, methylene chloride, water-immiscible esters, such as carboxylic acid dimethyl ester (dimethyl carbonate), ethyl formate, methyl, ethyl or isopropyl acetate; or water-immiscible ethers such as for example, methyl tert.butyl ether, and the like.
- halogenated aliphatic hydrocarbons such as for example, methylene chloride
- water-immiscible esters such as carboxylic acid dimethyl ester (dimethyl carbonate), ethyl formate, methyl, ethyl or isopropyl acetate
- water-immiscible ethers such as for example, methyl tert.butyl ether, and the like.
- the process in accordance with the invention provides a very efficient mixing or dispersing process for liquids.
- the mixing or dispersing process in accordance with the invention is also suitable for performing chemical reactions having very short reaction times, for example on the order of seconds or fractions of seconds.
- the mixing device in accordance with the invention has, in contrast to the known devices described above, an arrangement of the bores of the inlet and outlet nozzles which is axially spaced apart relative to one another.Thus, by the turbulence chamber being positioned between the nozzles, the short term stability of mixtures, especially of dispersions, is increased. This results in a liquid dispersion that is homogenized more strongly.
- a supply container ( 1 ) is followed by a high pressure pump ( 2 ) which is optionally connected to a heat exchanger ( 3 ).
- the mixing device ( 4 ) is positioned thereafter.
- FIG. 2 and FIG. 3 show a mixing device ( 4 ) consisting of an inlet nozzle ( 6 ) having a bore diameter of about 0.05 mm to about 1 mm, preferably about 0.05 mm to about 0.5 mm; a turbulence chamber ( 7 ) having a diameter of about 0.5 mm to about 10 mm, preferably about 1 mm to about 10 mm, such as about 1 mm to about 5 mm; an outlet nozzle ( 8 ) having a bore diameter of about 0.05 mm to about 1.5 mm, preferably about 0.05 mm to about 0.8 mm, with the inlet nozzle ( 6 ), the turbulence chamber ( 7 ) and the outlet nozzle ( 8 ) being pressed in sequence in a cylindrical support ( 5 ).
- the inlet nozzle is in fluid communication with the outlet nozzle via the turbulence chamber.
- the bores of the nozzles are axially spaced apart relative to one another.
- fluid communication is intended to mean that liquids to be mixed or dispersed enter the turbulence chamber through the bore of the inlet nozzle. Once in the turbulence chamber, the liquids are mixed and then exit the chamber via the bore of the outlet nozzle.
- the bores of the nozzles are said to be axially spaced apart relative to one another.
- the bores of the inlet and outlet nozzles are positioned on opposite sides of the axis of the chamber.
- the ratio of length to diameter of each nozzle bore amounts in the case of the inlet nozzle or the outlet nozzle to about 1 to 10, preferably about 1 to 5.
- the ratio of length to diameter of the turbulence chamber is about 0.5 to about 50, preferably about 0.5 to about 20, such as about 0.5 to about 10.
- the diameter of the turbulence chamber must be greater than the diameter of the outlet nozzle.
- the bore diameters of the inlet nozzle and the outlet nozzle may be the same or different. However, an embodiment in which the bore diameter of the inlet nozzle is smaller than the bore diameter of the outlet nozzle is preferred.
- the bore diameter of the inlet nozzle is about 0.2 mm and the bore diameter of the outlet nozzle is about 0.25 mm.
- the nozzles are suitably manufactured from wear-resistant materials such as e.g. sapphire, diamond, stainless steel, ceramic, silicon carbide, tungsten carbide, zirconium, and the like.
- the bores of the nozzles may be round, rectangular, or elliptical.
- a bore which has a cone in the mouth is also suitable.
- the cylindrical support ( 5 ) likewise consists of wear-resistant materials, suitably of stainless steel.
- FIG. 4 shows one possibility for the scale up of the mixing device.
- Section 4 a shows a plurality of nozzles in accordance with the invention with nozzle inserts ( 11 ), which are secured to a support plate ( 10 ).
- the nozzle inserts may be secured to the support plate by any conventional means, such as for example, they may be screwed into the support plate.
- the support plate is positioned in a conduit ( 9 ) (cylindrical support).
- Cross section 4 b shows only one nozzle insert ( 11 ′).
- the nozzle insert ( 11 ′), the support plate ( 10 ) as well as the conduit ( 9 ) are manufactured from wear-resistant materials, preferably stainless steel.
- Section 4 c shows the screwable nozzle support ( 11 ′′) which contains the nozzle ( 4 c ) in accordance with the invention.
- FIG. 5 shows another scale up arrangement.
- the mixing device consisting of a support disk ( 12 ), a turbulence chamber ( 13 ) and a support disk ( 14 ), which are positioned in sequence in a tubular conduit ( 15 ), with the first support disk ( 12 ) containing a plurality of inlet nozzles ( 16 ) having a bore diameter of about 0.05 mm to about 1 mm, preferably about 0.05 mm to about 0.5 mm, and the second support disk ( 14 ) containing a plurality of outlet nozzles ( 17 ) having a bore diameter of about 0.05 mm to about 1 mm, preferably about 0.05 mm to about 0.8 mm.
- the bores of the inlet nozzles are in fluid communication with the bores of the outlet nozzles through the turbulence chamber and the bores of the inlet nozzles and outlet nozzles are axially spaced apart relative to one another.
- the number of nozzles determines the diameter of the turbulence chamber ( 13 ).
- the ratio of length to diameter of the turbulence chamber is designed such that the residence time of a liquid to be dispersed in the dispersing unit is about 10 ⁇ 6 sec to about 10 ⁇ 1 sec.
- a pre-emulsion is first produced in the supply container ( 1 ) in a known manner and pumped through the dispersing unit ( 4 ) at temperatures of about 20° C. to about 250° C., preferably about 20° C. to about 200° C., and pressures of about 50 bar to about 2500 bar, preferably about 50 bar to about 800 bar, using a high pressure pump ( 2 ).
- the pre-emulsion may be heated for a brief period in the heat exchanger ( 3 ).
- the residence time of the liquid to be dispersed in the dispersing unit ( 4 ) is about 10 ⁇ 6 sec to about 10 ⁇ 1 sec.
- the emulsion had the following composition: 87 wt. % deionized water, 10 wt. % corn oil, and 3 wt. % lauryl ethylene oxide-9.
- Deionized water was placed in a kettle and warmed to 40° C.
- the emulsifier lauryl ethylene oxide (LEO)-9 was dissolved in the water.
- the corn oil was stirred in and comminuted with an ULTRA TURRAX mixer at 1000 rpm.
- the content of dispersed phase was 10 wt. %
- the weight ratio of corn oil to lauryl ethylene oxide was 10:3.
- the pre-emulsion was homogenized three times at a pressure of 600 bar using the dispersing unit set forth in FIG. 2 in accordance with the invention.
- the geometric dimensions of the dispersing units used are set forth in Table 1.
- the particle sizes were determined in a known manner by means of photon correlation spectroscopy.
- Example 1 Deionized water was placed in a kettle and warmed to 40° C. Ascorbyl palmitate was dissolved in the water at pH values between seven and eight. The production of the pre-emulsion and the homogenization were carried out according to Example 1.
- a pre-emulsion was produced in accordance with Example 2.
- the content of the dispersed phase was 30 wt. %.
- the weight ratio of dl-alpha-tocopherol to ascorbyl palmitate was 10:1.
- the pre-emulsion was homogenized once at pressures of 100 bar, 200 bar, 300 bar, 400 bar and 500 bar using the dispersing unit in accordance with the invention shown in FIG. 2 .
- the deionized water was placed in a kettle and warmed to 60° C.
- the fish gelatine was dissolved in the water.
- the ascorbyl palmitate was dissolved in the aforementioned solution at pH values between seven and eight.
- the dispersed phase including dl-alpha-tocopherol and corn oil was stirred in as described in Example 1.
- the pre-emulsion was homogenized in accordance with Example 4.
- Examples 6-10 are comparative Examples using a single-hole nozzle.
- the pre-emulsion was produced in accordance with Example 1 and homogenized three times at a pressure of 600 bar in a single-hole nozzle.
- the single-hole nozzle had an acute angled inlet and outlet.
- the geometric dimensions of the single-hole nozzle are given in Table 1.
- the pre-emulsion was produced in accordance with Example 2 and homogenized in the manner described in EXAMPLE 6.
- the pre-emulsion was produced in accordance with Example 3 and homogenized in the manner described in Example 6.
- the pre-emulsion was produced in accordance with Example 4 and homogenized once in a single-hole nozzle as described in Example 6 at pressures of 100 bar, 200 bar, 300 bar, 400 bar and 500 bar.
- the particle size was determined in a known manner by means of laser diffraction spectrometry and photon correlation spectroscopy.
- the pre-emulsion was produced in accordance with Example 5 and homogenized once in a single-hole nozzle as described in Example 6 at pressures of 100 bar, 200 bar, 300 bar, 400 bar and 500 bar.
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Abstract
Description
TABLE 1 |
Geometric dimensions of the dispersing units used. |
Length of | ||||
Bore diameter | Bore diameter | the | Bore diameter | |
of the inlet | of the | turbulence | of the | |
Nozzle | nozzle | turbulence | chamber | outlet nozzle |
type | [mm] | chamber [mm] | [mm] | [mm] |
Nozzle I | 0.2 | 2 | 1.5 | 0.25 |
Nozzle I | 0.2 | 2 | 3 | 0.28 |
long | ||||
Nozzle II | 0.2 | 2 | 1.5 | 0.2 |
Single- | 0.2 | — | — | — |
hole | ||||
nozzle | ||||
TABLE 2 |
Average particle sizes in nm of |
Passage 1 | Passage 2 | Passage 3 | ||
Example | Nozzle type | Particle size | Particle size | Particle size |
1 | Nozzle I | 218 | 202 | 202 |
0.2/0.25 mm | 219 | 215 | 200 | |
1 | Nozzle II | 230 | 214 | 212 |
0.2/0.2 mm | 231 | 220 | 208 | |
6 | single-hole | 307 | 256 | 247 |
nozzle | 298 | 250 | 248 | |
0.2 mm | ||||
2 | Nozzle I | 275 | 250 | 238 |
0.2/0.25 mm | ||||
2 | Nozzle II | 294 | 266 | 245 |
0.2/0.2 |
||||
7 | single-hole | 340 | 320 | 275 |
nozzle | ||||
0.2 mm | ||||
3 | Nozzle I | 295 | 287 | 267 |
0.2/0.25 mm | ||||
3 | Nozzle II | 312 | 294 | 302 |
0.2/0.2 |
||||
8 | single-hole | 442 | 416 | 403 |
nozzle | ||||
0.2 mm | ||||
TABLE 3 |
Average particle sizes in nm of |
100 bar | 200 bar | 300 bar | 400 bar | 500 bar | ||
Particle | Particle | Particle | Particle | Particle | ||
Nozzle | size | size | size | size | size | |
Ex. | type | [nm] | [nm] | [nm] | [nm] | [nm] |
4 | Nozzle I | 1800 | 1370 | 1400 | 1105 | 1080 |
0.2/0.25 | ||||||
mm | ||||||
4 | Nozzle | 1370 | 740 | 745 | 660 | 600 |
I/long | ||||||
0.2/0.28 | ||||||
|
||||||
9 | Single-hole | 5200 | 3080 | 1520 | 1370 | 914 |
nozzle | ||||||
0.2 mm | ||||||
5 | Nozzle I | 435 | 410 | 340 | 350 | 345 |
0.2/0.25 | ||||||
mm | ||||||
5 | Nozzle | 420 | 410 | 360 | 325 | 290 |
I/long | ||||||
0.2/0.28 | ||||||
|
||||||
10 | Single-hole | 440 | 430 | 360 | 350 | 355 |
nozzle | ||||||
0.2 mm | ||||||
Claims (7)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/174,178 US6536940B1 (en) | 1998-12-07 | 2002-06-18 | Preparation of liquid dispersions |
US10/355,833 US6722780B2 (en) | 1998-12-07 | 2003-01-31 | Preparation of liquid dispersions |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP98123237 | 1998-12-07 | ||
EP98123237 | 1998-12-07 |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/174,178 Division US6536940B1 (en) | 1998-12-07 | 2002-06-18 | Preparation of liquid dispersions |
US10/355,833 Division US6722780B2 (en) | 1998-12-07 | 2003-01-31 | Preparation of liquid dispersions |
Publications (1)
Publication Number | Publication Date |
---|---|
US6530684B1 true US6530684B1 (en) | 2003-03-11 |
Family
ID=8233099
Family Applications (3)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US09/455,135 Expired - Lifetime US6530684B1 (en) | 1998-12-07 | 1999-12-06 | Preparation of liquid dispersions |
US10/174,178 Expired - Lifetime US6536940B1 (en) | 1998-12-07 | 2002-06-18 | Preparation of liquid dispersions |
US10/355,833 Expired - Lifetime US6722780B2 (en) | 1998-12-07 | 2003-01-31 | Preparation of liquid dispersions |
Family Applications After (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/174,178 Expired - Lifetime US6536940B1 (en) | 1998-12-07 | 2002-06-18 | Preparation of liquid dispersions |
US10/355,833 Expired - Lifetime US6722780B2 (en) | 1998-12-07 | 2003-01-31 | Preparation of liquid dispersions |
Country Status (12)
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---|---|
US (3) | US6530684B1 (en) |
EP (1) | EP1008380B1 (en) |
JP (1) | JP2000167368A (en) |
KR (1) | KR100685540B1 (en) |
CN (1) | CN1128658C (en) |
AT (1) | ATE261336T1 (en) |
BR (1) | BR9907453A (en) |
CA (1) | CA2291565A1 (en) |
DE (1) | DE69915434T2 (en) |
DK (1) | DK1008380T3 (en) |
ES (1) | ES2216423T3 (en) |
IN (1) | IN189920B (en) |
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- 1999-12-02 ES ES99123878T patent/ES2216423T3/en not_active Expired - Lifetime
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Cited By (20)
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US20070211570A1 (en) * | 2000-04-20 | 2007-09-13 | Manfred Schauerte | Static mixing element and method of mixing a drilling liquid |
US7878705B2 (en) * | 2000-04-20 | 2011-02-01 | Tt Schmidt Gmbh | Static mixing element and method of mixing a drilling liquid |
US6953396B2 (en) * | 2000-10-23 | 2005-10-11 | Rite-Hite Holding Corporation | Fabric flow restriction and method for conveying a volume of air |
US20030194965A1 (en) * | 2000-10-23 | 2003-10-16 | Paschke Nicolas B. | Fabric flow restriction and method for conveying a volume of air |
US20090073801A1 (en) * | 2004-11-17 | 2009-03-19 | Basf Aktiengesellschaft | Process and device for producing finely divided liquid-liquid formulations, and the uses of the liquid-liquid formulations |
US20090003123A1 (en) * | 2007-06-28 | 2009-01-01 | Morrison Jr Lowen Robert | Apparatus and method for mixing by producing shear and/or cavitation, and components for apparatus |
US8517595B2 (en) * | 2007-06-28 | 2013-08-27 | The Procter & Gamble Company | Apparatus and method for mixing by producing shear and/or cavitation, and components for apparatus |
US20090199656A1 (en) * | 2008-02-12 | 2009-08-13 | Sunita Rani | Systems and methods for managing pressure and flow rate |
US9038669B2 (en) * | 2008-02-12 | 2015-05-26 | Sunita Rani | Systems and methods for managing pressure and flow rate |
US8759278B2 (en) | 2010-01-13 | 2014-06-24 | The Procter & Gamble Company | Method of producing a fabric softening composition |
US20130186493A1 (en) * | 2012-01-24 | 2013-07-25 | United Technologies Corporation | Bi-directional fluid flow regulator with funnel shaped baffles |
WO2013121295A3 (en) * | 2012-02-17 | 2013-12-19 | Wiab Water Innovation Ab | Mixing device |
US20130215709A1 (en) * | 2012-02-17 | 2013-08-22 | Bengt Olle Hinderson | Mixing device |
US9878293B2 (en) * | 2012-02-17 | 2018-01-30 | SoftOx Solutions AS | Mixing device |
US20180147548A1 (en) * | 2012-02-17 | 2018-05-31 | SoftOx Solutions AS | Mixing device |
US10906014B2 (en) * | 2012-02-17 | 2021-02-02 | Wiab Water Innovation Ab | Mixing device |
US20140319401A1 (en) * | 2013-04-29 | 2014-10-30 | Delavan Inc | Directionally biased valve |
US20180058695A1 (en) * | 2013-04-29 | 2018-03-01 | Delavan Inc. | Directionally biased valve |
US10240792B2 (en) * | 2013-04-29 | 2019-03-26 | Delavan Inc. | Directionally biased valve |
US20170056846A1 (en) * | 2014-05-09 | 2017-03-02 | Dow Global Technologies Llc | Static mixer |
Also Published As
Publication number | Publication date |
---|---|
ATE261336T1 (en) | 2004-03-15 |
KR100685540B1 (en) | 2007-02-22 |
EP1008380A3 (en) | 2000-12-13 |
CA2291565A1 (en) | 2000-06-07 |
US6722780B2 (en) | 2004-04-20 |
EP1008380B1 (en) | 2004-03-10 |
US6536940B1 (en) | 2003-03-25 |
CN1256168A (en) | 2000-06-14 |
EP1008380A2 (en) | 2000-06-14 |
DE69915434D1 (en) | 2004-04-15 |
US20030053372A1 (en) | 2003-03-20 |
DK1008380T3 (en) | 2004-07-12 |
CN1128658C (en) | 2003-11-26 |
DE69915434T2 (en) | 2005-03-03 |
JP2000167368A (en) | 2000-06-20 |
BR9907453A (en) | 2001-01-16 |
IN189920B (en) | 2003-05-10 |
US20030133355A1 (en) | 2003-07-17 |
KR20000057041A (en) | 2000-09-15 |
ES2216423T3 (en) | 2004-10-16 |
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